Process and apparatus for adiabatic fractionation



Feb. 25, 1947. w. PROELL 2,416,404

PROCESS AND APPARATUS FOR ADIABATIC FRACTIONATION Filed Aug. 23, 1943 2 Sheets-Sheet l Disfi/lafe FRACTION/1 7'//VG COLUMN FQBO Bo f/oms I v [n venfor Wayne A. Proe/l Afforney Feb. 25, 1947. w PROELL 2,416,404 PROCESS AND APPARATUS FOR ADIABATIC FRACTIONATION Filed.Aug. 23, 1943 zsheets-sheet 2 Disfi/lafe 1 .2 Dlsflllafe Z \\jja 10 Feed fnven/or' Wayne ,4. Proel/ Boffoms y gma e Af/orney Patented Feb. 25, 1947 UNITED STATES" PATENT :OFFICE PROCESS AND'APPABATUS FOB ADIABATIO FRACTIONATION of Indiana Application AW 23, 1943, Serial No. 499,649.

1 This invention relates to a process and apparatus for fractionation and more particularly relates to a fractionation system having automatic means for maintaining adiabatic conditions to efiect the separation of otherwise difllculty separable mixtures. The invention is particularly useful in the removal of traces of undesirable components of widely different boiling point from a given material or in the separation of components from a mixture wherein the boiling points of the several components are so close as to preclude eflicient separation by conventional means. An object of this invention is to provide a process and apparatus whereby a substantially adiabatic fractionation is effected. A further object is to provide a process and apparatus wherein a portion of the charge is utilized to maintain the system under substantially adiabatic conditions. Another object is to provide a method and means whereby a more eflicient fractionation is possible while obtaining a heat economy. Still another object of my invention is to provide a system whereby increased eiii ciencyin the separation of narrow boiling cuts is obtained. It is also an object of my invention to provide a wholly automatic system which provides a jacket of iiowing vapor having substantially the same composition as the desired'prod uct. Another object is to provide a method and means for the easy elimination of non-condensible gases. An additional object is to provide a method and means for adiabatic fractionation wherein smaller amounts of reflux are needed. These and other objects will become apparent as the description of my invention proceeds.

Referring to Figure 1 of the drawings, the apparatus is made up ofan innercolumn l which is a conventional fractionatlng column containing either bubble trays or other suitable packing I I preferably made of a heat conducting material, such as Wire gauze. The inner fractionating column In is jacketed by the outer shell l2, the bottom 25 of column l0 and the outer shell l2 communicating with a common or joint liquid reservoir l3. The shell I2 is closed to the atmosphere and the overhead therefrom is conducted by valved line l4 into a condenser or reflux drum l5 which is provided with the conventional cooling coils (not shown) through which may be passed a suitable cooling medium, a vent ll and condensate return line I6. A control valve 26 on line H regulates the vapor flow through the vapor jacket or shell I2 about the column Ill. Valve 26 may be manually set to dis- 5 Claims. (01. 195-94) charge a measured volume of vapor per hour .to

condenser ll, orit may be thermally controlled by a suitable thermostat to open only when the temperature falls below a selected temperature. Likewise means can be provided for controlling the valve 28 in response to the pressureexlsting disposed in the top of column ID. A bottom drawofi 24 is provided for the reservoir l3 which within the shell l2. In general, the valve 28 will be set at a small constant discharge rate with the object of preventing light ends accumulating in shell l2. Valve is as illustrated is pressure controlled to vent freely all noncondensible gases from the system and is provided with adjustable means. such as spring loading, to permit operation at any desired pressure ranging from atmospheric to superatmospheric. When the operation is under superatmospheric pressure, noncondensibles accumulated in the condenser are vented by valve l9 at the selected operating pres-' sure. This valve can bei thermostatically controlled to vent cold gases.

In the lower portion of the shell l2'a heating element 20 is immersed in the reservoir of liquid. This heating element is illustrated as a pipe coil supplied with a heating fluid, but it should be understood that the liquid may be withdrawn from the reservoir l3 and passed through a reboiler and reintroduced into the shell I! at a point below the bottom of column l0. Conduit means 2| is provided for introducing a feed into the column ll)" and overhead conduit 22 communicates with column I 0 for withdrawing the desired distillate. A cooling coil 23 to provide reflux is forms the bottom of the shell I? and communicates directly with the open bottom 25 of the column l0.

In operation, the hot ieed enters through conduit 2!, the lighter constituents of the vapor ascending through column l0 and undergoing fractionation therein. The heavier constituents pass downwardly through the column "I and are accumulated as bottoms in reservoir 13. Simultaneously heat is supplied to reservoir l3 and vapors therefrom ascend the shell or jacket l2 and provide an insulating envelope of vapor about the column In at a temperature substantially equal to that within the column [0. Concur-' rently a portion of the vapors enters the column it through the open bottom 25. By suitable throttling of valve 26, manually or automatically, controlled amounts of the vapor are continually removed from the shell l2 and condensed to I keep the space between the column I0 and the into the column l and/or the'amount of conden-' sation occurring in shell I2. For example, the

amount of reflux, the rate of vapor withdrawal from the shell l2 and the amount or heat introduced by reboiler means 20 can be so correlated that there is substantially no condensation of the. vapor on the wall of column I 0, but that sufficient additional heat is supplied by the reboiler to compensate for the normal heat loss to the atmosphere by the condensation of a portion of the vapor'upon shell l2. Thus an adiabatic temperature control is provided when the cut being fractionated has a narrow boiling range or contains traces of heavier contaminants. The vapor from shell i2 passes through valve 26 in line l4 and the heavier constituents are liquefled in condenser IS. The valve I9 is used as a pressure control for the system and as a vent valve for the non-condensible gases withdrawn from the condenser IS. The liquid from condenser i is recycled by line IE to the reservoir i3 in the bottom of shell l2.

It will be apparent that the narrower the out being fractionated, the more eflicient the column will be since' its overall temperature then approaches a constant and approaches perfect adiabaticity. Consequently my invention is particularly adapted to the fractionation of such mixtures as isomeric butene, heptane-toluene, and toluene-xylene'mixtures, and the like. In view of its adiabatic nature the column is well adapted to the use of highly efllcient packings of low flooding capacity, such as the type wherein wire gauze cones are disposed apex to apex and base to base with larger openings being provided for the upward passage of vapor in contact with the capil- 4 lary film of reflux liquid which is supported by the wire gauze.

For the lighter petroleum products, suchas gasoline constituents, esters, pure hydrocarbons and the like, more eflicient fractionation is desiroverhead from annular iractionating tower I2 is conducted therefrom by line H. In the lower portion of the apparatus reservoir i3 is provided with a heating element 20 immersed in the pool of liquid. A bottom drawofl 24- is provided for the reservoir .i3 whichforms the bottom of the annular fr tion tin column l2 and communicates directly with the open bottom 25 of the column Ill. The overhead from each of the fractionating zones is withdrawn by lines 14 and 22, passed through coolers and 3i, and introduced into reflux drums 32 and 33, respectively. Reflux drum 33 is provided with a vent line 34 having valve 42 which may be used to control the pressure of the system and to vent the non-condensible gases from the condenser 33. A portion of the liquid from condenser 33 can-be withdrawn as a desired distillate by line 35 and another portion returned by line 36 to column i0 as reflux. Alternatively the column I0 may be provided with'a cooling coil near its top to provide the necessary reflux liquid. The overhead from shell 12 is withdrawn through line It, cooler 30 and introduced to reflux drum 32. ,The overhead from reflux drum 32 is withdrawn by valved line 31 and introduced into condenser 33, for example by line 22 or valve 43 in line 31 may be closed and'noncondensible gases may be vented from drum 32 via valved vent 4|. A portion of the liquid from reflux drum 32 is introduced by line 38 and distributor 39 as reflux for fractionating tower l2. Another portion of the liquid may be withdrawn by line 40 as a desired distillate.

able. Small scale fractionating columns are useful as analytical apparatus and in the design and operation of large scale equipment. In small scale operations, however, heat losses usually render the fractionation far from adiabatic. My invention is particularly useful in eliminating heat losses from this type of column to attain the desired fractionation control but it is contemplated that it can..be applied to full' plant scale operation.

Figure 2 illustrates another embodiment of the invention wherein the elements corresponding to those of Figure 1 are identified by similar reference characters. Thus an inner column Ill and an outer shell I2 are provided and have packing I H and Ila similar to that proposed for Figure 1. The inner fractionating column in is surrounded by the outer or annular fractionating tower I 2,

' the bottom of column Ill and the annular tower i2 communicating with a common or joint liquid reservoir l3. Conduit means 2| is provided for introducing a vapor feed into the column i0 and overhead conduit 22 communicates with column ID for withdrawing a desired distillate. The

In operation of the apparatus illustrated in Figure 2 the hot mixed feed vapors enter through conduit 2|, the lighter constituents of the vapors ascending through the column l0 and undergoing fractionation therein. The heavier constituents pass downwardly through the column i0 and are accumulated as bottoms in reservoir l3. Simultaneously heat is supplied to the reservoir i3 and vaporized hydrocarbons ascend the annular fractionating tower 12 thereby providing an insulating envelope about the column Ill. Concurrently a portion of the vapors enters the column I!) through the open bottom 25. One fraction is recovered by line 3-5 and another by line 40, drawofis 44 and 65 being closed in this operation. By controlling the relative rates of reflux supplied to column l0 and the shell i2 by line 36 or 38, along with the heat input to reservoir [3 a unique and efllcient fractionating system is provided. The fractionating column i0 is substantially adiabatic and the. product recovered therefrom will be substantially free of any contaminants which comprise either traces of high. boiling materials or hydrocarbons which have boiling points approaching that of the desired distillate. Thus I.

tha with the removal of the heavy color produc- I ing bodies. Likewise mixtures of toluene, xylene and normal heptane can be separated to produce substantially pure toluene. When the light constituent is to be substantially pure the mix is introduced by line 2| as shown. When the heavier constituent is to be recovered the mix is introduced directly into shell l2.

The apparatus of Figure 2 also may be modified and employed in the separation and recovery of azeotropic mixtures. Thus an aromaticparafiln mixture with an azeotropic agent can be introduced by line 2!, drums 32 and 33 operated as separators, parafiins recovered by draw- 01,! lines 44 and/or 45, aromatics at 24, and the agent recycled as reflux by lines 38 and 38.

From the above it will apparent that I have attained the objects of myinvention and have shell, means for maintaining a vapor pressure said column, a shell substantially surroundingsaid column, means for accumulating a pool of liquid in the lower portion of said shell, the bottom of said fractionating column having direct vapor communication with the vapor space above said pool, means for supplying heat to the liquid in said pool, valve means responsive to conditions within the shell for controllably withdrawing vapor from said shell at a high point therein, means for. condensing said vapors exterior of said shell, means for returning at least a portion of said condensate to said pool, means for withdrawing from said column a selected component of said mixture, and means for withdrawing a second component from said shell.

2. The apparatus of claim 1 wherein said valve means is controlled by the pressure within the shell.

'3. The apparatus of claim 1 whichincludes a vent from said means for condensing vapors, said vent comprising a valve thermostatically controlled by the temperature of the non-condensible gases therein.

4. Fractionating apparatus comprising an inner Iractionating column, a shell substantially surrounding said column, means for accumulating a pool of liquid below said iractionating column and shell, said shell and said fractionating column being in direct vapor communication with the-vapor space above'said pool, means for withhead on said condenser, means for venting uncondensable gases from said condenser means, a conduit directly connecting said condenser means to said pool-accumulating means for returning condensate from said condenser means to said pool, and means for withdrawing a selected component from a high point in said column.

5. Apparatus for fractionating a narrow boiling mixture comprising an inner fractionating column, a conduit means for introducing said narrow boiling mixture into said fractionating column at an intermediate point, a shell substantially surrounding said column, means for accumulating a pool of liquid in the lower por-- tion of said shell, the lower end of said fractionating column being in direct vapor communica! tion with the vapor space above said pool, means for supplying heat to the liquid in said pool, means for controllably withdrawing vapor from said shell at a high point therein, means for condensing at least a portion of said withdrawn vapors exterior of said shell, a conduit directly connecting said condensing means to said poolaccumulating means for returning condensate from said condensing means to said pool, means I for withdrawing from said condensing means an drawing vapor from said shell at a high point therein,.condenser means exterior of said' shell and i'ractionating column for condensing atleast' aportion or said vapors withdrawn from said uncondensed vapor fraction, and means for withdrawing from a high point in said column selected component of said mixture.

WAYNE A. PRO ELL.

REFERENCES crran 1 The following references are of record in the flle of this patent:

UNITED sums PATENTS Number 1 v Name Date 2,281,906 Adams May 5, 1942 1,318,657 Frasch Oct. '14, 1919 1,086,452 Golodetz Feb. 10, 1914 1,804,553 Dubbs May 12, 1931 2,070,100 Twomey Feb.'9. 1937 1,759,813 Gray May 20, 1930 1,865,474 Mandelbaum July 5, 1932 FOREIGN PATENTS- Number Country Date 795,827 France Jan. 13, 1936 

